CN110165177A - A kind of silicon-based composite anode material for Li-ion battery - Google Patents
A kind of silicon-based composite anode material for Li-ion battery Download PDFInfo
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- CN110165177A CN110165177A CN201910428409.6A CN201910428409A CN110165177A CN 110165177 A CN110165177 A CN 110165177A CN 201910428409 A CN201910428409 A CN 201910428409A CN 110165177 A CN110165177 A CN 110165177A
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M4/362—Composites
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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Abstract
The invention discloses a kind of silicon-based composite anode material for Li-ion battery, Si, amorphous SiO of the composite material by amorphous/nanocrystallinexAnd Cu3Si composition of alloy；Its preparation step are as follows: Si and CuO powder is added according to Si:CuO=1 ~ 39:2 mol ratio in ball grinder, ball mill is placed in the state of protective atmosphere and carries out ball milling generation solid-state reaction, obtains Si@SiOx/Cu3Si silicon-based composite anode material for Li-ion battery.Si@SiO of the inventionx/Cu3Si composite lithium ion battery cathode material has the characteristics that simple process, cycle performance are excellent and capacity is high.
Description
Technical field
The present invention relates to technical field of lithium ion battery negative, specifically a kind of novel lithium ion battery silicon substrate is multiple
Condensation material system.
Background technique
Lithium ion battery has great strategic importance in new energy field, is the hot spot technology of current generation.Cathode material
The selection of Material system and its performance are to determine one of the key factor of performance of lithium ion battery of new generation.Traditional commercialized carbon
The problem of capacity of negative electrode material has reached the limit, essence is the low (372mAhg of the theoretical capacity of carbon material-1).
In view of this, U.S. patent Nos US7972727B2 discloses ELECTRODE COMPOSITIONS BASFD ON
AN AMORPHOUS ALLOY HAVING A HIGH SILICON CONTENT, is related to Si-Al composite negative pole material, have compared with
High specific capacity, Si55Al29.3Fe15.7Specific capacity reach 1400 mAhg-1, still, alloy material of cathode is use process
Middle pulverizing problem is inevitable, and volume expansion is big, causes biggish obstacle to practical application.
In numerous non-carbon negative material systems studied, Si system (3580 mAhg of high capacity-1) it is to have existed
Small range realizes the lithium ion battery negative material of application and Sustainable Exploitation, is the research heat of novel anode material in recent years
Point.But studies have shown that negative electrode material of the Si as lithium ion battery, because the huge volume expansion of Si causes electrode failure and nothing
Method obtains good cycle performance.
For in this respect, Chinese invention patent application CN1402366A discloses a kind of negative electrode of lithium ion battery Fabrication of High Specific Capacitance
The Si-C composite material and preparation method of amount, the composite material are existed by siliceous class lithium storage materials as main active substances
In composite material, and dispersible carrier of the carbon with easy, the reversible embedding de- lithium performance of storage lithium as active material, composite wood
Material general formula is Si-C-X, and the content of siliceous active material is 10%- after active material and dispersible carrier high temperature solid state reaction
50% (wt), the specific capacity for the composite negative pole material prepared are much higher than carbons negative electrode material commonly used at present, circulation
Service life is much better than alloy system.But this method is still without solving the problems, such as volume expansion.
Summary of the invention
It is of the invention it is main be designed to provide a kind of novel silicon substrate composite lithium ion battery cathode material, have
The feature that simple process, cycle performance are excellent and capacity is high.
The present invention can be achieved through the following technical solutions:
The invention discloses a kind of new type lithium ion battery silicon substrate composite negative pole material composite materials by amorphous/nanocrystalline
Si, amorphous SiOxAnd Cu3Si composition of alloy, wherein the value of x is 0≤x≤2.After ball milling, the composite material being prepared is
Micro nano structure, wherein amorphous SiOx and Cu3Si is generated in-situ.
Further, the composite negative pole material is the preparation using mechanical alloying method.Relative to other synthesis sides
Method, mechanical alloying method is more easy, and yield is high, and the material granule size of preparation is thinner.
Further, the mechanical alloying method is planetary type ball-milling or shimmy formula ball-milling method.Ball-milling technology is simple, ring
It protects, yield is high, and industrialization is with the obvious advantage.
Further, the specific preparation step of composite negative pole material are as follows: according to Si:CuO=1 ~ 39:2 in ball grinder
Si and CuO powder is added in mol ratio, and ball mill is placed in the state of protective atmosphere and carries out ball milling generation solid-state reaction, is obtained
To Si@SiOx/Cu3Si silicon-based composite anode material for Li-ion battery.The composite material being prepared is micro nano structure, wherein
Amorphous SiOx and Cu3Si is generated in-situ.
Further, the protective atmosphere is the inert gas not reacted with silicon.
Further, the inert gas is nitrogen, argon gas and/or helium.The composite material being prepared is micro-nano
Structure, wherein amorphous SiOx and Cu3Si is generated in-situ.
Further, in mechanical milling process, ratio of grinding media to material is 10~80:1.Ratio of grinding media to material is too small, then soldering degree between reactant
Not enough, can not further refining composite material, ratio of grinding media to material is excessive, then wastes experiment consumptive material, higher cost.
Si@SiO of the present inventionx/Cu3Si composite lithium ion battery cathode material has following beneficial technical effect:
The first, the capacity controllable of material can efficiently control silicon de- by adjusting the different accountings of silicon in the composite
Cubical expansivity in process of intercalation；
The second, cycle performance is excellent, which is by amorphous Si, amorphous SiOxAnd Cu3Si composition of alloy,
Middle x indicates oxygen content,.Wherein generated in-situ amorphous SiOxAnd its Cu3Si is not only to the refinement journey of Si
Degree improves, and at the same time having had both the oxide of silicon and its advantage of silicon-base alloy system, delays to a certain extent
Volume expansion of silicon during removal lithium embedded is solved, to greatly improve the cycle performance of lithium ion battery；
Third, capacity are high, gained Si@SiOx/Cu3Si composite lithium ion battery cathode material is as negative electrode of lithium ion battery material
Material, compared to other negative electrode materials, the characteristics of having taken into account high capacity and good cycle；
4th, preparation process is simple, gained Si@SiOx/Cu3The preparation method of Si composite lithium ion battery cathode material is simple,
No pollution to the environment.
Detailed description of the invention
Attached drawing 1 is the Si@SiO that different material ratio is prepared by shimmy formula ball millingx/Cu3Si composite lithium ion cell
Negative electrode material XRD spectra (embodiment 1,2,4,6)；
Attached drawing 2 is the Si@SiO prepared by mechanical alloying methodx/Cu3The SEM of Si composite lithium ion battery cathode material schemes
(embodiment 4)；
Attached drawing 3 is Si@SiOx/Cu3Si composite lithium ion battery cathode material charge and discharge by voltage be 0.005V~1.5V
(vs. Li+/ Li), charging and discharging currents density is 0.4mA cm-2Under the conditions of first time, second of charging and discharging curve (embodiment
4)；
Attached drawing 4 is Si@SiOx/Cu3Cycling behavior figure (embodiment 4) in Si composite lithium ion battery cathode material；
Attached drawing 5 is Si@SiOx/Cu3Coulombic efficiency figure (embodiment 4) in Si composite lithium ion battery cathode material.
Attached drawing 6 is the Si@SiO that planetary type ball-milling is preparedx/Cu3Si composite lithium ion battery cathode material XRD spectra
(embodiment 5)；
Attached drawing 7 is XRD spectrum (embodiment 5) of composite material under the conditions of 0.05C after lithiumation.
Specific embodiment
In order that those skilled in the art will better understand the technical solution of the present invention, below with reference to embodiment and to this
Invention product is described in further detail.
The invention discloses a kind of new type lithium ion battery silicon substrate composite negative pole material composite materials by amorphous/nanocrystalline
Si, amorphous SiOxAnd Cu3Si composition of alloy, wherein the value of x is 0≤x≤2.After ball milling, the composite material that is prepared
For micro nano structure, wherein amorphous SiOx and Cu3Si is generated in-situ.
Further, the composite negative pole material is the preparation using mechanical alloying method.
Further, the mechanical alloying method is planetary type ball-milling or shimmy formula ball-milling method.
Further, the specific preparation step of composite negative pole material are as follows: according to Si:CuO=1 ~ 39:2 in ball grinder
Si and CuO powder is added in mol ratio, and ball mill is placed in the state of protective atmosphere and carries out ball milling generation solid-state reaction, is obtained
To Si@SiOx/Cu3Si silicon-based composite anode material for Li-ion battery.The composite material being prepared is micro nano structure, wherein
Amorphous SiOx and Cu3Si is generated in-situ.
Further, the protective atmosphere is the inert gas not reacted with silicon.
Further, the inert gas is nitrogen, argon gas and/or helium.The composite material being prepared is micro-nano
Structure, wherein amorphous SiOx and Cu3Si is generated in-situ.
Further, in mechanical milling process, ratio of grinding media to material is 10~80:1.
In the present invention, the time of ball milling specific Binding experiment condition is controlled, and 2~200h is involved in the present invention
Time range, in a particular embodiment not one by one and foot illustrate.
Embodiment 1
The invention discloses a kind of novel silicon substrate composite lithium ion battery cathode material composite material be by amorphous Si,
Amorphous SiOxAnd Cu3Si composition of alloy, wherein the value of x is 0≤x.Preparation method is mechanical alloying method, mainly includes
Planetary type ball-milling, shimmy formula ball milling.The following steps are included: Si is added according to the mol ratio of Si:CuO=5:2 in ball grinder
With CuO powder, it is placed on shimmy formula ball mill in the state of protective atmosphere and carries out ball milling generation solid-state reaction, obtains Si@
SiOx/Cu3Si composite lithium ion battery cathode material.
In the present embodiment, shimmy formula ball mill carries out ball milling.The protective atmosphere is argon gas.The ball grinder and ball
Ball milling pearl its medium in grinding jar is stainless steel.In mechanical milling process, ratio of grinding media to material 15:1.
Embodiment 2
The present embodiment and the difference of embodiment 1 are: in the present embodiment, shimmy formula ball mill carries out ball milling.The protection gas
Atmosphere is argon gas.Its medium of the ball grinder and in ball grinder ball milling pearl is stainless steel.In mechanical milling process, ratio of grinding media to material is
30:1。
Embodiment 3
The present embodiment and the difference of embodiment 1 are: in the present embodiment, planetary ball mill carries out ball milling.The protection gas
Atmosphere is helium.Its medium of the ball grinder and in ball grinder ball milling pearl is stainless steel.In mechanical milling process, ratio of grinding media to material is
50:1。
Embodiment 4
The present embodiment and the difference of embodiment 1 are: in the present embodiment, shimmy formula ball mill carries out ball milling.The protection gas
Atmosphere be argon gas and.Its medium of the ball grinder and in ball grinder ball milling pearl is stainless steel.In mechanical milling process, ratio of grinding media to material is
60:1。
Embodiment 5
The present embodiment and the difference of embodiment 1 are: in the present embodiment, planetary ball mill carries out ball milling.The protection gas
Atmosphere is nitrogen and helium.Its medium of the ball grinder and in ball grinder ball milling pearl is stainless steel.In mechanical milling process, ball material
Than for 60:1.
Embodiment 6
The present embodiment and the difference of embodiment 1 are: in the present embodiment, shimmy formula ball mill carries out ball milling.The protection gas
Atmosphere is nitrogen and helium.Its medium of the ball grinder and in ball grinder ball milling pearl is stainless steel.In mechanical milling process, ball material
Than for 80:1.
In order to verify the performance of resulting materials of the present invention, it is prepared into half-cell in accordance with the following methods and is tested: by ball
Si@SiO after millx/Cu3Si composite powder, conductive agent super-p and binder LiPAA 85:2:13 in mass ratio are uniformly mixed
Coated on being fabricated to electrode slice on copper foil.In argon atmosphere glove box, using lithium metal as to electrode, ethylene carbonate (EC)
+ dimethyl carbonate (DMC)+vinyl fluoride carbonate (FEC)+1MLiPF6For electrolyte, it is assembled into button cell and is tested.It surveys
Strip part are as follows: charging and discharging currents density is 0.4mAhcm-2, charge and discharge are 0.005V~1.5V (vs. Li by voltage+/ Li),
As a result as shown in Fig. 1~5.
By solid phase reduction method, Si@SiO has been prepared in we as seen from Figure 1x/Cu3Si composite material, and silicon
Crystallinity decrease, this shows silicon that ball milling obtains, and some is converted into amorphous state.
Preparing resulting composite material as seen from Figure 2 is micro nano structure, and entire material is by different nanoparticle institutes
It constitutes, helps to alleviate silicon volume expansion during removal lithium embedded.
Ratio is that 19:2 prepares resulting Si@SiO as seen from Figure 3x/Cu3Its first discharge specific capacity of Si composite material
Up to 1918mAh/g, irreversible capacity is about 530mAh/g or so for the first time.
Ratio is that 19:2 prepares resulting Si@SiO as seen from Figure 4x/Cu3Si composite material circulation 50 times after,
Capacity is about 450mAh/g, and for pure silicon, cycle performance has biggish promotion.
Ratio is that 19:2 prepares resulting Si@SiO as seen from Figure 5x/Cu3Si composite material its coulombic efficiency is for the first time
72% or so, its coulombic efficiency shows good cycle performance 99% or so after stablizing.
Silicon particle is further refined as can see from Figure 6, has most silicon to be converted into amorphous state.Amorphous
The silicon of state plays a significant role inhibition volume expansion due to the characteristic of itself structure.
There is no Li in process of intercalation in silicon as can see from Figure 715Si4Amorphous state is also just not present in the process of crystallization
LixSiyWith crystalline state Li15Si4Two-phase coexistent area.Since two-phase section is related with high internal stress, there is no two-phase coexistent areas to show this
Composite material effectively inhibits the volume expansion of silicon.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the present invention in any form；It is all
The those of ordinary skill of the industry can be shown in by specification and described above and swimmingly implement the present invention；But it is all familiar
Professional and technical personnel without departing from the scope of the present invention, makes using disclosed above technology contents
A little variation, modification and evolution equivalent variations, be equivalent embodiment of the invention；Meanwhile all realities according to the present invention
The variation, modification and evolution etc. of matter technology any equivalent variations to the above embodiments, still fall within technology of the invention
Within the protection scope of scheme.
Claims (6)
1. a kind of silicon-based composite anode material for Li-ion battery, it is characterised in that: the composite material by amorphous/nanocrystalline Si,
Amorphous SiOxAnd Cu3Si composition of alloy, wherein the value of x is 0≤x≤2.
2. silicon-based composite anode material for Li-ion battery according to claim 1, it is characterised in that: the composite negative pole material
It is the preparation using mechanical alloying method.
3. silicon-based composite anode material for Li-ion battery according to claim 2, it is characterised in that: the mechanical alloying method
For planetary type ball-milling or shimmy formula ball-milling method.
4. the silicon-based composite anode material for Li-ion battery according to Claims 2 or 3, it is characterised in that: composite negative pole material
Specific preparation step are as follows: in ball grinder according to Si:CuO=1 ~ 39:2 mol ratio be added Si and CuO powder, protecting
It is placed on ball mill in the state of atmosphere and carries out ball milling generation solid-state reaction, obtains Si@SiOx/Cu3Si lithium ion battery silicon substrate is multiple
Close negative electrode material.
5. silicon-based composite anode material for Li-ion battery according to claim 4, it is characterised in that: the protective atmosphere be with
The inert gas that silicon does not react.
6. silicon-based composite anode material for Li-ion battery according to claim 5, it is characterised in that: the inert gas is nitrogen
Gas, argon gas and/or helium.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112885997A (en) * | 2020-04-23 | 2021-06-01 | 郑州轻工业大学 | Preparation method and application of novel silicon-based composite porous negative electrode material of lithium ion battery |
| CN113213483A (en) * | 2021-04-14 | 2021-08-06 | 三峡大学 | Preparation method of amorphous silicon powder for lithium ion battery cathode material |
| CN114597375A (en) * | 2022-03-21 | 2022-06-07 | 南京径祥新材料科技有限公司 | Silicon-based negative electrode composite material of lithium ion battery, preparation method and lithium ion battery |
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| CN1930726A (en) * | 2004-03-16 | 2007-03-14 | 松下电器产业株式会社 | Lithium secondary battery |
| CN103682279A (en) * | 2013-12-27 | 2014-03-26 | 浙江大学 | Silicon-based composite lithium ion battery negative electrode material as well as preparation method and application of silicon-based composite lithium ion battery negative electrode material |
| CN104995772A (en) * | 2013-03-30 | 2015-10-21 | 国立大学法人东北大学 | Negative electrode active material for lithium ion secondary batteries, method for producing same, negative electrode, and battery |
| CN106159246A (en) * | 2015-03-31 | 2016-11-23 | 中国科学院金属研究所 | A kind of siliceous porous amorphous alloy lithium ion battery negative material and preparation method thereof |
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2019
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1930726A (en) * | 2004-03-16 | 2007-03-14 | 松下电器产业株式会社 | Lithium secondary battery |
| CN104995772A (en) * | 2013-03-30 | 2015-10-21 | 国立大学法人东北大学 | Negative electrode active material for lithium ion secondary batteries, method for producing same, negative electrode, and battery |
| CN103682279A (en) * | 2013-12-27 | 2014-03-26 | 浙江大学 | Silicon-based composite lithium ion battery negative electrode material as well as preparation method and application of silicon-based composite lithium ion battery negative electrode material |
| CN106159246A (en) * | 2015-03-31 | 2016-11-23 | 中国科学院金属研究所 | A kind of siliceous porous amorphous alloy lithium ion battery negative material and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112885997A (en) * | 2020-04-23 | 2021-06-01 | 郑州轻工业大学 | Preparation method and application of novel silicon-based composite porous negative electrode material of lithium ion battery |
| CN112885997B (en) * | 2020-04-23 | 2022-02-15 | 郑州轻工业大学 | Preparation method and application of novel silicon-based composite porous negative electrode material of lithium ion battery |
| CN113213483A (en) * | 2021-04-14 | 2021-08-06 | 三峡大学 | Preparation method of amorphous silicon powder for lithium ion battery cathode material |
| CN114597375A (en) * | 2022-03-21 | 2022-06-07 | 南京径祥新材料科技有限公司 | Silicon-based negative electrode composite material of lithium ion battery, preparation method and lithium ion battery |
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